Hydrochloric Acid → HCID 11660878, 화합물

HRID 2192195노트

반응식

HRID 2192195 반응식
[NH2:1][C:2]1[CH:19]=[C:18]([F:20])[C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]3[NH:13][CH:14]=[C:15]([C:16]#[N:17])[C:8]=23)=[C:4]([F:21])[CH:3]=1.Cl[C:23]1[CH:28]=[CH:27][N:26]=[C:25]([NH2:29])[N:24]=1.Cl.[OH-].[Na+]>O.C(O)C>[NH2:29][C:25]1[N:26]=[C:27]([NH:1][C:2]2[CH:19]=[C:18]([F:20])[C:5]([O:6][C:7]3[CH:12]=[CH:11][N:10]=[C:9]4[NH:13][CH:14]=[C:15]([C:16]#[N:17])[C:8]=34)=[C:4]([F:21])[CH:3]=2)[CH:28]=[CH:23][N:24]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 2233322-Amino-4-chloropyrimidineHCID 59740983HCID 59740983, 화합물

생성물 1

HCID 11660878HCID 11660878, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

250 mg (0.65 mmol) of 4-(4-amino-2,6-difluorophenoxy)-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile and 92 mg (0.71 mmol) of 4-chloropyrimidine-2-amine are suspended in 10 ml of water and 5 ml of ethanol. 0.32 ml (1.29 mmol) of 4N hydrochloric acid is added, and the mixture is heated at reflux for 2 h. The mixture is made alkaline using concentrated aqueous sodium hydroxide solution, diluted with water and extracted with ethyl acetate. The organic phase is separated off and concentrated. The crude product is purified by preparative HPLC. This gives the title compound as crystals.

후처리

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 2 h
  3. extractionextracted with ethyl acetate
  4. customThe organic phase is separated off
  5. concentrationconcentrated
  6. customThe crude product is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-96da8a147eb0402082ce02d18d729319
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329716B2

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